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6-Methylpyridine-2-carboxylic acid → HCID 44539828、化合物

HRID 1695793
ノート
印刷プレビュー

反応式

HRID 1695793 の反応式
ClC(N(C)C)=C(C)C.[CH3:9][C:10]1[N:15]=[C:14]([C:16]([OH:18])=O)[CH:13]=[CH:12][CH:11]=1.[NH2:19][C:20]1[CH:28]=[C:27]([C:29]2[CH:30]=[C:31]([NH:36][S:37]([CH3:40])(=[O:39])=[O:38])[C:32]([Cl:35])=[N:33][CH:34]=2)[CH:26]=[C:25]2[C:21]=1[CH:22]=[N:23][N:24]2[CH3:41].C(=O)(O)[O-].[Na+]>C(Cl)Cl>[Cl:35][C:32]1[N:33]=[CH:34][C:29]([C:27]2[CH:26]=[C:25]3[C:21]([CH:22]=[N:23][N:24]3[CH3:41])=[C:20]([NH:19][C:16]([C:14]3[CH:13]=[CH:12][CH:11]=[C:10]([CH3:9])[N:15]=3)=[O:18])[CH:28]=2)=[CH:30][C:31]=1[NH:36][S:37]([CH3:40])(=[O:39])=[O:38]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 702826-Methylpyridine-2-carboxylic acidHCID 516892Sodium BicarbonateHCID 6407921-Chloro-N,N-2-trimethylpropenylamineHCID 86653304HCID 86653304、化合物

生成物 1

HCID 44539828HCID 44539828、化合物収率 6%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒
4 回

実験手順

1-Chloro-N,N,2-trimethyl-1-propen-1-amine (0.042 ml) was added to 6-methyl-2-pyridinecarboxylic acid (44 mg) in DCM (1 ml). The reaction was stirred at RT for 20 mins. N-[5-(4-Amino-1-methyl-1H-indazol-6-yl)-2-chloro-3-pyridinyl]methanesulfonamide (75 mg) in DCM (2 ml) was added and the reaction stirred for 30 mins. Approximately 4 ml saturated sodium bicarbonate (aq) was added followed by DCM (3 ml). The reaction was stirred vigorously. The DCM was passed through a hydrophobic frit then evaporated to dryness. The residue was dissolved in DMSO:methanol (1 ml, 1:1, v/v) and purified by MDAP (method E). The pure fraction was evaporated to dryness to give title compound (6 mg)

後処理

  1. stirringthe reaction stirred for 30 mins
  2. stirringThe reaction was stirred vigorously
  3. customthen evaporated to dryness
  4. dissolutionThe residue was dissolved in DMSO
  5. custommethanol (1 ml, 1:1, v/v) and purified by MDAP (method E)
  6. customThe pure fraction was evaporated to dryness

出典と根拠

ORDレコード
ord-89c4728f3106400da076ae4dcd23cb16
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08163743B2

反応ノート

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